Abstract
Cyclohexylammonium hexaisothiocyanatonickelate(II) dihydrate, (C6H11NH3)4[Ni(NCS)6]·2H2O, was synthesized, for the first time, by a four-step method in a yield of 95%. The compound was fully characterized by elemental microanalysis, Fourier transform infrared (FTIR), ultraviolet-visible-near infrared (UV-Vis-NIR), and nuclear magnetic resonance (NMR) spectroscopy and thermogravimetry. A single crystal X-ray diffraction (SXRD) gave the monoclinic space group P21/c with a = 15.8179 (5) Å, b = 10.6222 (3) Å, c = 13.8751 (4) Å, β = 109.362 (1)°, V = 2199.45 (11) Å3, Z = 2 (T = 293 K) for this novel hybrid organic–inorganic compound. The title compound was employed as a single-source precursor for the synthesis of mesoporous, high surface area nickel oxide (53 Å; 452 m2/g) and nickel sulfide (46 Å; 220 m2/g) via pyrolysis under air at 550 °C or helium atmosphere at 500 °C, respectively. X-ray powder diffraction (XRPD) demonstrated the nanocrystalline nature of both NiO and NiS with an average crystallite size of 16 and 54 nm, respectively. Scanning electron microscope (SEM) indicated the formation of agglomerated, quasi-spherical particles of nickel oxide and agglomerated flake-like structures of nickel sulfide. The high surface area, porosity, and nanocrystallinity of both NiO and NiS, obtained via this approach, are promising for a wide spectrum of applications.
Highlights
For more than 100 years, the triatomic linear thiocyanate [SCN]− or isothiocyanate [NCS]− ligand has captured the attention of many researchers due to its low toxicity and varied coordination modes to metal ions
Fourier transform infrared (FTIR) spectrophotometry verified the formation of the target hybrid organic–inorganic compound, which was confirmed by UV-Vis-NIR absorbance and single-crystal X-ray diffraction (SCXRD)
~1.0 eV between each two successive absorption bands, we could assign the ν3 transition to ligand–metal charge transfer (LMCT) because it was the strongest in terms of energy and intensity, ascribe the ν2 transition to ligand field (d-d) band, and attribute the ν1 transition to both of d-d and LMCT, where part of LMCT is symmetrically banned for the perfectly octahedral hexaisothiocyanatonickelate(II) and feebly permitted in the real distorted structure of this complex, and ν1 transition was observed stronger and more intense than ν2 transition
Summary
For more than 100 years, the triatomic linear thiocyanate [SCN]− or isothiocyanate [NCS]− ligand has captured the attention of many researchers due to its low toxicity and varied coordination modes to metal ions. On the basis of the organic cation, cyclohexylammonium is a unique building block due to its capability to form various dimensional structures, depending on the identity of its counter anion and the presence of solvent of crystallization molecules, via its hydrogen donor nature [14,15,16,17,18,19,20,21,22,23,24,25,26,27,28,29,30,31,32,33,34,35,36,37] Another attractive feature of cyclohexylammonium is its usefulness as a soft organic template for the creation of mesopores, after its thermal decomposition, within the produced ceramic [26,38,39]. (C6 H11 NH3 )4 [Ni(NCS)6 ]·2H2 O was synthesized, characterized, and utilized as an SSP, via its thermal decomposition under two different atmospheres, for high surface area, mesoporous, nanocrystalline nickel sulfide (NiS) and nickel oxide (NiO)
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